CN115594883A - Method for separating and utilizing waste cotton-polyester blended fabric based on acidic hydrogen peroxide solution - Google Patents
Method for separating and utilizing waste cotton-polyester blended fabric based on acidic hydrogen peroxide solution Download PDFInfo
- Publication number
- CN115594883A CN115594883A CN202211206921.4A CN202211206921A CN115594883A CN 115594883 A CN115594883 A CN 115594883A CN 202211206921 A CN202211206921 A CN 202211206921A CN 115594883 A CN115594883 A CN 115594883A
- Authority
- CN
- China
- Prior art keywords
- cotton
- polyester
- hydrogen peroxide
- peroxide solution
- blended fabric
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J11/00—Recovery or working-up of waste materials
- C08J11/04—Recovery or working-up of waste materials of polymers
- C08J11/10—Recovery or working-up of waste materials of polymers by chemically breaking down the molecular chains of polymers or breaking of crosslinks, e.g. devulcanisation
- C08J11/16—Recovery or working-up of waste materials of polymers by chemically breaking down the molecular chains of polymers or breaking of crosslinks, e.g. devulcanisation by treatment with inorganic material
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2301/00—Characterised by the use of cellulose, modified cellulose or cellulose derivatives
- C08J2301/08—Cellulose derivatives
- C08J2301/26—Cellulose ethers
- C08J2301/28—Alkyl ethers
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2367/00—Characterised by the use of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Derivatives of such polymers
- C08J2367/02—Polyesters derived from dicarboxylic acids and dihydroxy compounds
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2401/00—Characterised by the use of cellulose, modified cellulose or cellulose derivatives
- C08J2401/08—Cellulose derivatives
- C08J2401/26—Cellulose ethers
- C08J2401/28—Alkyl ethers
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2467/00—Characterised by the use of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Derivatives of such polymers
- C08J2467/02—Polyesters derived from dicarboxylic acids and dihydroxy compounds
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/62—Plastics recycling; Rubber recycling
Landscapes
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Sustainable Development (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Separation, Recovery Or Treatment Of Waste Materials Containing Plastics (AREA)
- Processing Of Solid Wastes (AREA)
Abstract
The invention relates to a method for separating and utilizing waste polyester-cotton blended fabrics based on an acidic hydrogen peroxide solution, which utilizes the acidity and the oxidability of the acidic hydrogen peroxide solution, selectively hydrolyzes and oxidizes cotton fibers in the polyester-cotton blended fabrics into powdery oxidized cellulose through hydrothermal reaction, peels the oxidized cellulose from polyester fibers, simply, quickly and efficiently separates the polyester fibers and the cotton fibers, and synchronously realizes the oxidation modification of the cotton fibers and the direct recycling of the polyester fibers.
Description
Technical Field
The invention relates to a component separation and comprehensive utilization method of waste polyester-cotton blended fabrics, belonging to the technical field of waste textile recycling.
Background
The polyester-cotton blended fabric is widely applied to the textile industry due to good performance, and is the textile type with the largest use amount at present. With the importance of China on reasonable treatment and resource utilization of waste textiles, high-value recycling of waste cotton-polyester blended fabrics is concerned. The efficient component separation of the polyester fiber and the cotton fiber is the key for high-value recycling of waste polyester-cotton mixed textiles.
The existing physical opening and carding mode easily causes fiber fracture and damage, is used for separating polyester fibers and cotton fibers with high difficulty, and is difficult to effectively and simply realize polyester-cotton separation and recycling. According to the difference of the physical and chemical properties of the polyester fiber and the cotton fiber, a single component is dissolved or degraded by a chemical method, and the other component is recovered, so that the original form and physical and chemical properties of the components can be kept as much as possible in the recovery process.
Wherein, the breakage of glycosidic bond is easy to happen to the cotton fiber under the acid condition, which causes the depolymerization and chain breakage of macromolecular polymer, the fiber form is destroyed, and the terylene fiber is more stable to the reaction condition, can keep the fiber form, and the physical and chemical properties change little. Therefore, in the prior art, the cotton fiber is degraded, the fiber form of the cotton fiber is damaged, the cotton fiber is stripped from the polyester fiber, the polyester fiber is directly recovered, and the component separation of the polyester-cotton blended fabric is realized.
For example, CN 107245128 a uses sulfuric acid treatment and mechanical pulverization to change cotton fiber into powder while retaining the polyester fiber, during the mechanical pulverization process, the polyester fiber group floats on the upper layer by the centrifugal force of the pulverizer, and the cotton fiber powder sinks on the bottom layer, separating the polyester fiber group and the cotton fiber powder. However, the mechanical properties of the polyester fibers are impaired under the action of the machine, so that the subsequent application of the polyester fibers is limited. CN 106674588A discloses a method for recycling waste cotton-polyester blended fabrics under subcritical water conditions, which mainly uses dilute hydrochloric acid as a reactant and ferric chloride as a catalyst to obtain microcrystalline cellulose and terylene under subcritical conditions. The microcrystalline cellulose powder is easy to adhere to the terylene recovered by the method, and the purity of the recovered terylene is lower.
CN 112409635A carries out dilute acid pretreatment, NMMO aqueous solution dissolution, cellulase in-situ hydrolysis and solid-liquid separation on waste polyester-cotton fabric in sequence to obtain enzyme hydrolysis liquid and high-purity low-loss terylene. The method combines chemical, physical and biological methods, realizes the high-efficiency separation of the terylene and the cotton fiber, has less mass loss of the terylene in the regeneration process, does not contain any impurity on the surface of the recovered terylene, still can maintain the original mechanical property and thermal property, but has expensive price of the used NMMO and cellulase and higher treatment cost.
CN 109467741A adopts hydrothermal reaction catalyzed by organic acid to separate and recycle waste polyester-cotton textiles, the cotton fiber is degraded under the catalysis of the organic acid in a high-pressure reactor, and after the polyester fiber aggregate is filtered out, the rest part is cleaned to obtain cotton fiber fragments. The cellulose separated by the method has different polymerization degrees, is not beneficial to direct application, and mostly needs further modification treatment.
The oxidized cellulose is used as a derivative of cellulose, has good biocompatibility and biodegradability and no toxicity, can be applied to the preparation of high-performance membrane materials, and is suitable for various fields such as water treatment, biomedical materials, novel batteries and the like. At present, chemical pretreatment methods such as a TEMPO reagent and a periodate reagent are mainly used at home and abroad to realize the oxidation treatment of cotton pulp cellulose, but the methods may generate various toxic and harmful intermediate products in the reaction process.
CN 108727507A extracts cellulose from corncobs, and after the cellulose is prepared into a cellulose solution, oxidation treatment is carried out by using a TEMPO reagent to obtain oxidized cellulose. The obtained oxidized cellulose is in a spherical structure, has the particle size of 20-30 nm, and has good amphipathy and strong emulsibility.
CN 104017090A uses hydrogen peroxide to oxidize cellulose to prepare carboxyl cellulose, through pretreatment solution soaking, washing, suction filtration to neutrality, adding catalyst and oxidant hydrogen peroxide to carry out oxidation treatment, then solid-liquid separation, washing to neutrality, drying to obtain oxidized cellulose with different oxidation degrees. But different cellulose sources have different oxidation effects on the oxidation system.
Therefore, a simple, rapid and environment-friendly method for realizing efficient separation of components in waste cotton-polyester blended fabrics so as to obtain directly applicable cellulose products and high-purity polyester fibers at the same time is urgently needed to be researched.
Disclosure of Invention
The invention aims to provide a method for separating waste polyester-cotton blended fabrics by using an acidic hydrogen peroxide solution, which is used for simply, quickly and efficiently separating polyester fibers and cotton fibers and synchronously realizing the oxidation modification of cotton cellulose and the direct recycling of the polyester fibers.
In order to achieve the aim, the invention provides a method for separating and utilizing waste cotton-polyester blended fabrics based on an acidic hydrogen peroxide solution, which comprises the following steps:
1) Cleaning the waste cotton-polyester blended fabric, removing impurities and drying;
2) Soaking the washed cotton-polyester blended fabric into an acidic hydrogen peroxide solution for sufficient wetting, and heating the cotton-polyester blended fabric to 100-160 ℃ in a high-pressure reaction container for hydrothermal reaction;
3) Carrying out ultrasonic treatment on the hydrothermal reaction mixture, separating out residual fabrics, washing and drying to obtain polyester fibers;
4) And carrying out solid-liquid separation on the residual hydrothermal reaction mixture, collecting a solid product, washing and drying to obtain the oxidized cellulose.
Wherein the acidic hydrogen peroxide solution is prepared by adding inorganic acid into conventional 1-30% hydrogen peroxide solution to provide acidic environment, and adding H into the acidic hydrogen peroxide solution + The concentration is 0.1-1.2mol/L.
Generally, the inorganic acid may include, but is not limited to, any one of conventional inorganic acids such as hydrochloric acid, sulfuric acid, phosphoric acid.
The invention has no special requirement on the dosage of the acidic hydrogen peroxide solution for wetting the cotton-polyester blended fabric, as long as the cotton-polyester blended fabric can be completely soaked in the acidic hydrogen peroxide solution.
Generally, the polyester-cotton blended fabric is preferably immersed in the acidic hydrogen peroxide solution for sufficient wetting according to the solid-liquid mass volume ratio of the polyester-cotton blended fabric to the acidic hydrogen peroxide solution of 1.
Further, the hydrothermal reaction of the present invention preferably takes 0.5 to 8 hours.
The ultrasonic treatment of the hydrothermal reaction mixture aims at completely separating oxidized cellulose solid particles obtained by degrading cotton fibers from residual fabrics so as to obtain purer polyester fibers.
Further, the ultrasonic treatment is preferably ultrasonic treatment at a power of 100W and a frequency of 65Hz for 5-60min.
Furthermore, the solid-liquid separation method of the residual hydrothermal reaction mixture in the present invention is not particularly limited, and may be any conventional solid-liquid separation method, for example, filtration separation or centrifugal separation.
The method utilizes the acidity and the oxidability of the acidic hydrogen peroxide solution to hydrolyze the polyester-cotton blended fabric under a mild condition, selectively hydrolyze and oxidize cotton fibers in the polyester-cotton blended fabric, destroy the fiber morphology of the cotton fibers, hydrolyze the cotton fibers into powdery oxidized cellulose, and strip the oxidized cellulose from the polyester fibers.
Furthermore, the oxidized cellulose modified by oxidation has a large amount of carboxyl, and is beneficial to falling off from polyester fiber, so that the efficient separation of polyester-cotton components can be realized; the oxidized cellulose obtained after the oxidative degradation of the cotton fiber does not need further modification treatment, and can be directly applied to the aspects of wastewater treatment, carrier materials, functional materials, reinforcing materials and the like.
The oxidant hydrogen peroxide used in the invention has low price and good oxidation effect, and the decomposition product is water and carbon dioxide, thereby avoiding the use of toxic, harmful and large-irritation chemical reagents, and being safe and environment-friendly. Therefore, the invention provides a green, environment-friendly and effective method for realizing component separation and cellulose oxidation modification and recycling of waste cotton-polyester blended fabrics in one step.
Drawings
FIG. 1 is an SEM image of a waste cotton-polyester blended fabric used as a raw material in examples.
FIG. 2 is an SEM image of the separated polyester fibers in the example.
FIG. 3 is a FTIR plot of oxidized cellulose and cellulose after degradation in the examples.
Detailed Description
The following detailed description of embodiments of the present invention is provided in connection with the accompanying drawings and examples. The following examples are only for more clearly illustrating the technical solutions of the present invention so as to enable those skilled in the art to better understand and utilize the present invention, and do not limit the scope of the present invention.
Unless otherwise indicated, the production processes, experimental methods or detection methods related to the embodiments of the present invention are all conventional methods in the prior art, and the names and/or abbreviations thereof all belong to conventional names in the art, and are also clearly and clearly defined in the related fields of use, and those skilled in the art can understand the conventional process steps and apply corresponding equipment according to the names to implement the processes according to the conventional conditions or conditions suggested by manufacturers.
The various instruments, equipment, materials or reagents used in the examples of the present invention are not particularly limited in their sources, and are all conventional products commercially available or may be prepared according to conventional methods known to those skilled in the art.
The waste cotton-polyester blended fabrics used for recycling in the examples and the comparative examples of the invention are the blended fabrics with the ratio of the cotton-polyester blended fabric of 65, the SEM image of the blended fabrics is shown in figure 1, and the SEM image clearly shows that the blended fabrics are formed by closely interweaving the polyester fibers and the cotton fibers together.
Example 1.
Respectively weighing 98wt% of concentrated H 2 SO 4 2.041g,30wt% H 2 O 2 16.7g of solution, addWas added to 81.259g of distilled water to prepare 100g of a solution containing 2% by weight of H 2 SO 4 And 5wt% H 2 O 2 Acid hydrogen peroxide solution of (2).
Cutting the waste cotton-polyester blended fabric into blocks, washing with water and drying.
Weighing 2g of blocky waste polyester-cotton blended fabric according to the solid-to-liquid ratio of 1.
And (3) carrying out ultrasonic treatment on the reaction mixture for 30min, filtering by using a filter screen, collecting solid matters, repeatedly washing with water and ethanol for multiple times respectively until the solid matters are neutral, and drying to obtain 1.3236g of the polyester fabric.
As can be seen by comparing the figure 2 with the figure 1, the polyester-cotton components in the treated fabric are effectively separated, only the polyester fibers exist in the fabric, and the cotton fibers are completely removed.
And (3) performing centrifugal separation on the filter residues, collecting precipitates, performing centrifugal washing for multiple times by using water until the precipitates are neutral, and drying to obtain 0.3402g of oxidized cellulose powder.
From the FTIR spectrum of FIG. 3, it can be seen that the product after treatment with acidic hydrogen peroxide solution was at 1728cm compared to microcrystalline cellulose -1 Obvious carboxyl absorption peak is shown, which indicates that the separation product contains carboxyl groups, and proves that the cotton fiber is hydrolyzed and oxidized into oxidized cellulose containing carboxyl groups.
Comparative example 1.
Weighing 30wt% of H 2 O 2 16.7g of the solution was added to 83.3g of distilled water to prepare a 5wt% hydrogen peroxide solution.
Cutting the waste cotton-polyester blended fabric into blocks, washing with water and drying.
Weighing 2g of blocky waste polyester-cotton blended fabric according to the solid-to-liquid ratio of 1.
And (3) carrying out ultrasonic treatment on the reaction product for 30min, filtering by using a filter screen, collecting a solid matter, repeatedly washing the solid matter with water and ethanol for multiple times respectively until the solid matter is neutral, and drying to obtain 1.9872g of fabric.
Compared with the example 1, the quality of the fabric treated by the method is only slightly changed, and the removal rate of the cotton fiber in the polyester-cotton blended fabric is very low, so that the effective separation of the two components of the polyester fiber and the cotton fiber cannot be realized.
The cotton fiber has the characteristics of high crystallinity and high polymerization degree, and the structure of the cotton fiber is difficult to damage only by the weak acidity of the hydrogen peroxide solution, so that the degradation rate of the cotton fiber is extremely low, and the separation of the cotton fiber and the polyester fiber cannot be realized.
Comparative example 2.
Weighing 30wt% of H 2 O 2 50g of the solution was added to 50g of distilled water to prepare a 15wt% hydrogen peroxide solution.
Cutting the waste cotton-polyester blended fabric into blocks, washing with water and drying.
Weighing 2g of blocky waste cotton-polyester blended fabric according to the solid-to-liquid ratio of 1.
And (3) carrying out ultrasonic treatment on the reaction product for 30min, filtering by using a filter screen, collecting solid matters, repeatedly washing the solid matters with water and ethanol for multiple times respectively until the solid matters are neutral, and drying to obtain 1.9834g of fabric.
Compared with the comparative example 1, although the quality of the fabric is slightly reduced, the removal rate of the cotton fiber is extremely low, and the fact that the structure of the cotton fiber is difficult to damage even a high-concentration hydrogen peroxide solution is achieved by simply depending on the oxidation of the hydrogen peroxide proves that the degradation rate of the cotton fiber is extremely low, and the effective separation of the cotton fiber and the polyester fiber cannot be realized.
Comparative example 3.
Weighing 98wt% of concentrated H 2 SO 4 2.041g of the resulting solution was added to 97.959g of distilled water to prepare a 2wt% dilute sulfuric acid solution.
Cutting the waste cotton-polyester blended fabric into blocks, washing with water and drying.
Weighing 2g of blocky waste cotton-polyester blended fabric according to the solid-to-liquid ratio of 1.
And (3) carrying out ultrasonic treatment on the reaction product for 30min, filtering by using a filter screen, collecting solid matters, repeatedly washing the solid matters with water and ethanol for multiple times respectively until the solid matters are neutral, and drying to obtain 1.3359g of the polyester fabric.
And (4) performing centrifugal separation on the filter residues, collecting precipitates, performing centrifugal washing for multiple times by using water to be neutral, and drying to obtain 0.3450g of cellulose powder.
As can be seen from the FTIR spectrum of fig. 3, the acid treated product was only slightly oxidized and its carboxyl content was significantly lower than the oxidized cellulose obtained after treatment with acidic hydrogen peroxide solution.
Compared with the embodiment 1, the component separation of the polyester fiber and the cotton fiber can be realized after the treatment of the embodiment, the polyester fiber is stained with a small amount of cellulose, the polyester fiber with higher purity can be obtained after the washing and the ultrasonic vibration treatment for many times, but the obtained cellulose powder is the cellulose which is not subjected to the oxidation modification treatment.
Comparative example 4.
Respectively weighing 98wt% of concentrated H 2 SO 4 0.1020g,30wt% of H 2 O 2 50g of the solution was added to 48.8980g of distilled water to prepare 100g of a solution containing 0.1wt% of H 2 SO 4 And 15wt% H 2 O 2 The acidic hydrogen peroxide solution of (1).
Cutting the waste cotton-polyester blended fabric into blocks, washing with water and drying.
Weighing 2g of blocky waste cotton-polyester blended fabric according to the solid-to-liquid ratio of 1.
And (3) carrying out ultrasonic treatment on the reaction mixture for 30min, filtering by using a filter screen, collecting solid matters, repeatedly washing the solid matters with water and ethanol for multiple times respectively until the solid matters are neutral, and drying to obtain 1.8771g of fabric.
And centrifugally separating the filter residues, collecting precipitates, centrifugally washing the precipitates to be neutral by water for multiple times, and drying the precipitates to obtain trace oxidized cellulose powder.
Compared with the example 1, the effective separation of the components of the polyester fiber and the cotton fiber can not be realized after the treatment, a large amount of cotton fiber is still remained on the surface of the polyester fiber, and only a trace amount of oxidized cellulose powder can be obtained, which proves that acid with a certain concentration in a treatment system is necessary because the cotton fiber has the characteristics of high crystallinity and high polymerization degree, and if the concentration of the acid is too low, the degradation rate of the cotton fiber is extremely low, so that the effective separation of the cotton fiber and the polyester fiber can not be realized.
Example 2.
Respectively weighing 98wt% of concentrated H 2 SO 4 2.041g,30wt% H 2 O 2 16.7g of the solution was added to 81.259g of distilled water to prepare 100g of a solution containing 2wt% of H 2 SO 4 And 5wt% H 2 O 2 The acidic hydrogen peroxide solution of (1).
Cutting the waste cotton-polyester blended fabric into blocks, washing with water and drying.
Weighing 2g of blocky waste cotton-polyester blended fabric according to the solid-to-liquid ratio of 1.
And (3) carrying out ultrasonic treatment on the reaction mixture for 30min, filtering by using a filter screen, collecting solid matters, repeatedly washing with water and ethanol for multiple times respectively until the solid matters are neutral, and drying to obtain 1.3528g of polyester fabric.
And (4) carrying out centrifugal separation on the filter residues, collecting precipitates, carrying out centrifugal washing for multiple times by using water until the precipitates are neutral, and drying to obtain 0.3285g of oxidized cellulose powder.
Analysis and determination show that the treated polyester-cotton components are effectively separated, the polyester is completely recovered, the mechanical property is good, and the cotton fiber is hydrolyzed and oxidized into oxidized cellulose containing carboxyl.
Example 3.
Respectively weighing 98wt% of concentrated H 2 SO 4 1.0205g,30wt% H 2 O 2 50g of the solution was added to 47.959g of distilled water to prepare 100g of a solution containing 1% by weight of H 2 SO 4 And 15wt% of H 2 O 2 The acidic hydrogen peroxide solution of (1).
Cutting the waste cotton-polyester blended fabric into blocks, washing with water and drying.
Weighing 2g of blocky waste cotton-polyester blended fabric according to the solid-to-liquid ratio of 1.
And (3) carrying out ultrasonic treatment on the reaction mixture for 60min, filtering by using a filter screen, collecting solid matters, repeatedly washing the solid matters with water and ethanol for multiple times respectively until the solid matters are neutral, and drying to obtain 1.3387g of the polyester fabric.
And (4) carrying out centrifugal separation on the filter residues, collecting precipitates, carrying out centrifugal washing for multiple times by using water until the precipitates are neutral, and drying to obtain 0.3357g of oxidized cellulose powder.
Analysis and determination show that the components of the treated polyester cotton are effectively separated, the polyester fiber is completely recovered and has good mechanical property, and the cotton fiber is hydrolyzed and oxidized into oxidized cellulose containing carboxyl.
Example 4.
Respectively weighing 98wt% of concentrated H 2 SO 4 3.0615g,30wt% H 2 O 2 50g of the solution was added to 46.9385g of distilled water to prepare 100g of a solution containing 3wt% of H 2 SO 4 And 15wt% H 2 O 2 Acid hydrogen peroxide solution of (2).
Cutting the waste cotton-polyester blended fabric into blocks, washing with water and drying.
Weighing 2g of blocky waste polyester-cotton blended fabric according to the solid-to-liquid ratio of 1.
And (3) carrying out ultrasonic treatment on the reaction mixture for 20min, filtering by using a filter screen, collecting solid matters, repeatedly washing the solid matters with water and ethanol for multiple times respectively until the solid matters are neutral, and drying to obtain 1.3192g of polyester fabric.
And (3) performing centrifugal separation on the filter residues, collecting precipitates, performing centrifugal washing for multiple times by using water to be neutral, and drying to obtain 0.2928g of oxidized cellulose powder.
Analysis and determination show that the components of the treated polyester cotton are effectively separated, the polyester fiber is completely recovered and has good mechanical property, and the cotton fiber is hydrolyzed and oxidized into oxidized cellulose containing carboxyl.
Example 5.
Respectively weighing 98wt% of concentrated H 2 SO 4 3.0615g,30wt% H 2 O 2 33.4g of the solution was added to 47.959g of distilled water to prepare 100g of a solution containing 3wt% of H 2 SO 4 And 10wt% of H 2 O 2 Acid hydrogen peroxide solution of (2).
Cutting waste cotton-polyester blended fabric into blocks, washing with water and drying.
Weighing 2g of blocky waste polyester-cotton blended fabric according to the solid-to-liquid ratio of 1.
And (3) carrying out ultrasonic treatment on the reaction mixture for 30min, filtering by using a filter screen, collecting solid matters, repeatedly washing the solid matters with water and ethanol for multiple times respectively until the solid matters are neutral, and drying to obtain 1.3955g of the polyester fabric.
And (4) carrying out centrifugal separation on the filter residues, collecting precipitates, carrying out centrifugal washing for multiple times by using water until the precipitates are neutral, and drying to obtain 0.3541g of oxidized cellulose powder.
Analysis and determination show that the components of the treated polyester cotton are effectively separated, the polyester fiber is completely recovered and has good mechanical property, and the cotton fiber is hydrolyzed and oxidized into oxidized cellulose containing carboxyl.
The above embodiments of the present invention are not intended to be exhaustive or to limit the invention to the precise form disclosed. Various changes, modifications, substitutions and alterations to these embodiments will be apparent to those skilled in the art without departing from the spirit and scope of the present invention.
Claims (7)
1. A method for separating and utilizing waste cotton-polyester blended fabric based on acidic hydrogen peroxide solution comprises the following steps:
1) Cleaning the waste cotton-polyester blended fabric, removing impurities and drying;
2) Soaking the washed cotton-polyester blended fabric into an acidic hydrogen peroxide solution for sufficient wetting, and heating the cotton-polyester blended fabric to 100-160 ℃ in a high-pressure reaction container for hydrothermal reaction;
3) Carrying out ultrasonic treatment on the hydrothermal reaction mixture, separating out residual fabrics, washing and drying to obtain polyester fibers;
4) Carrying out solid-liquid separation on the residual hydrothermal reaction mixture, collecting a solid product, washing and drying to obtain oxidized cellulose;
wherein, H of the acidic hydrogen peroxide solution + The concentration is 0.1-1.2mol/L.
2. The method as set forth in claim 1, wherein the H is obtained by adding an inorganic acid to a hydrogen peroxide solution having a mass concentration of 1 to 30% + 0.1-1.2mol/L of acidic hydrogen peroxide solution.
3. The method according to claim 2, wherein the inorganic acid is any one of hydrochloric acid, sulfuric acid and phosphoric acid.
4. The method as set forth in claim 1, wherein the cotton-polyester blended fabric is immersed in the acidic hydrogen peroxide solution for sufficient wetting according to the solid-liquid mass volume ratio of the cotton-polyester blended fabric to the acidic hydrogen peroxide solution being 1.
5. The method as set forth in claim 1, characterized in that the hydrothermal reaction time is 0.5-8h.
6. The method according to claim 1, wherein the ultrasonic treatment is at a power of 100W and a frequency of 65Hz for a period of 5-60min.
7. The method as set forth in claim 1, characterized in that the solid-liquid separation of the residual hydrothermal reaction mixture is filtration or centrifugation.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211206921.4A CN115594883B (en) | 2022-09-30 | 2022-09-30 | Method for separating and utilizing waste polyester-cotton blended fabric based on acidic hydrogen peroxide solution |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211206921.4A CN115594883B (en) | 2022-09-30 | 2022-09-30 | Method for separating and utilizing waste polyester-cotton blended fabric based on acidic hydrogen peroxide solution |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN115594883A true CN115594883A (en) | 2023-01-13 |
| CN115594883B CN115594883B (en) | 2023-09-29 |
Family
ID=84845189
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202211206921.4A Active CN115594883B (en) | 2022-09-30 | 2022-09-30 | Method for separating and utilizing waste polyester-cotton blended fabric based on acidic hydrogen peroxide solution |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN115594883B (en) |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104017090A (en) * | 2014-05-05 | 2014-09-03 | 华南理工大学 | Method for preparing carboxycellulose by using hydrogen peroxide |
| US20190218362A1 (en) * | 2018-01-12 | 2019-07-18 | Tyton Biosciences, Llc | Methods for recycling cotton and polyester fibers from waste textiles |
| US20200232162A1 (en) * | 2017-04-27 | 2020-07-23 | Infinited Fiber Company Oy | Treatment process for textile-based materials |
| CN112409635A (en) * | 2020-10-30 | 2021-02-26 | 东华大学 | Method for separating, recycling and utilizing waste polyester-cotton blended fabric |
-
2022
- 2022-09-30 CN CN202211206921.4A patent/CN115594883B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104017090A (en) * | 2014-05-05 | 2014-09-03 | 华南理工大学 | Method for preparing carboxycellulose by using hydrogen peroxide |
| US20200232162A1 (en) * | 2017-04-27 | 2020-07-23 | Infinited Fiber Company Oy | Treatment process for textile-based materials |
| US20190218362A1 (en) * | 2018-01-12 | 2019-07-18 | Tyton Biosciences, Llc | Methods for recycling cotton and polyester fibers from waste textiles |
| CN112409635A (en) * | 2020-10-30 | 2021-02-26 | 东华大学 | Method for separating, recycling and utilizing waste polyester-cotton blended fabric |
Also Published As
| Publication number | Publication date |
|---|---|
| CN115594883B (en) | 2023-09-29 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| EP2598535B1 (en) | Method for production of cellulose nano crystals from cellulose-containing waste materials | |
| CN101391844B (en) | Salting pickled vegetable brine recovery technique | |
| CN102321681B (en) | Method and device for preparing gallic acid | |
| CN112409635B (en) | Method for separating, recycling and utilizing waste polyester-cotton blended fabric | |
| CN107629245B (en) | Recycling method of waste polyester-cotton blended fabric under hydrothermal condition | |
| CN100522982C (en) | Production process for extracting tea saponin from tea-oil tree cake by using water as dissoluent | |
| CN102911395A (en) | Resourced recovering and utilizing method for waste cotton fabric | |
| JP2009001734A (en) | Method for decomposing cellulose-based mixed fiber/fabric, and resultant decomposed product | |
| CN115594883B (en) | Method for separating and utilizing waste polyester-cotton blended fabric based on acidic hydrogen peroxide solution | |
| CN111893789A (en) | Preparation method and application of nano fibrillated cellulose | |
| CN115417404B (en) | Method for preparing graphene oxide from waste graphene film scraps | |
| CN101649568A (en) | Environment-friendly method for extracting cellulose | |
| CN114874343B (en) | Spherical nanocrystalline cellulose based on furfural residues and preparation method thereof | |
| JP2009001733A (en) | Method for decomposing/liquefying solid cellulose, and resultant decomposed product | |
| CN115678943A (en) | Method for treating cotton-containing fabric waste | |
| CN102701963B (en) | Method for preparing potassium hydrogen terephthalate | |
| CN110105407A (en) | A method of degradation humic acid and ulmic acid are to prepare fulvic acid | |
| CN108586770B (en) | Method for cleaning and separating lignin and hemicellulose from plant biomass | |
| CN1067049C (en) | Process for producing terephthalic acid | |
| CN113880958A (en) | Method for preparing kelp residue nanocrystalline cellulose by using eutectic solvent and ultrasound | |
| CN117510977A (en) | Method for efficiently separating and recycling polyester-cotton blended fabric through electron beam irradiation pretreatment | |
| CN110627129B (en) | Method for removing polyester waste solution by magnetic fluid adsorption and chain decomposition | |
| JPH02184651A (en) | Method of recovering terephthalic acid | |
| CN116856188A (en) | Method for preparing cellulose fiber from camellia oleifera and typha and prepared cellulose fiber | |
| CN116815528A (en) | Lignin removing method for straw |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |